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Powders of oxide-ion conductor La2Mo2O9 presenting nanodomains were synthesized by using polyol processes. The influence of different process parameters on the structure and particles morphology was determined. By the classical polyol process, whatever the polyol solvent used (ethylene glycol, diethylene glycol, 1,2-propanediol and tetraethylene glycol) platelet particles with dimensions of few hundred nanometers long and around twenty nanometers thick were observed, as agglomerates of small sub-particles. Only with diethylene glycol, pure La2Mo2O9 was obtained, whereas with microwave assistance, ethylene glycol also leads to pure product. For both ethylene and diethylene glycol solvent, the microwave assisted process resulted in either agglomerates or desert roses conglomerates after heat treatments at 500 degrees C for 5 min or 2 h. Specific surface areas, ranging between 23 and 36 m(2) g(-1), have been measured for pure La2Mo2O9 powders. (C) 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.